CN107904410A - A kind of compound degasser prepares the production method of high temperature alloy and the special high-purity metal chromium of target - Google Patents
A kind of compound degasser prepares the production method of high temperature alloy and the special high-purity metal chromium of target Download PDFInfo
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- CN107904410A CN107904410A CN201711071630.8A CN201711071630A CN107904410A CN 107904410 A CN107904410 A CN 107904410A CN 201711071630 A CN201711071630 A CN 201711071630A CN 107904410 A CN107904410 A CN 107904410A
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- compound
- degasser
- chromium
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- reducing agent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
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- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Powder Metallurgy (AREA)
Abstract
A kind of compound degasser prepares the production method of high temperature alloy and the special high-purity metal chromium of target, after the crome metal piece that electrolysis produces is crushed, mixed with compound degasser graphite-like reducing agent and metal class desulfurization reducing agent, obtain mixture, mixture is pressed into billet, is then charged into square graphite material frame；Graphite material frame equipped with mixture billet is put into vacuum drying oven, is vacuumized, is started to warm up as vacuum≤5Mpa in vacuum drying oven, temperature rises to 1400 DEG C~1600 DEG C, cool down after insulation 29h~35h, come out of the stove, obtain the high-purity metal chromium product of chromium purity >=99.9%.Advantage is：Technique is simple, and using the crome metal piece of electrolysis production as raw material, appearance is in the form of sheets, be conducive to the progress of reaction, using compound degasser, preferably can remove the elemental gas in raw material, product impurity element is extremely low and uniform quality, can meet the requirement of high temperature alloy and high-end target.
Description
Technical field
The present invention relates to one kind using crome metal piece as raw material, using compound degasser production high-purity metal chromium method, this
Kind high-purity metal chromium metal impurities are (such as：Iron, aluminium, silicon) and gaseous impurity is (such as：Oxygen, sulphur, nitrogen) it is extremely low, it is high temperature alloy and top grade
The dedicated basic material of target industry.
Background technology
High-purity metal chromium extensively should due to having the characteristics that molten boiling point is high, hardness is big, high temperature resistant, anticorrosive, good toughness
For fields such as metallurgy, electronics, Aeronautics and Astronautics, mainly for the production of high temperature alloy, target, in addition, it may also be used for make accurate
Electronic product, display, video screen and advanced optical material film plating.In recent years, it is fast with China's aerospace cause
Speed development, it is increasing to the demand of high temperature alloy and target domain-specific high-purity metal chromium, but due to such to high pure metal
The impurity content of chromium requires stringenter, it is desirable to which high-purity metal chromium purity is high, impurity content is low, and the main chemical compositions of product need to reach
To following index：Cr ＞ 99.9%, Fe ＜ 0.02%, Al ＜ 0.01%, Si ＜ 0.01%, C ＜ 0.012%, O ＜ 0.03%,
Especially to elemental gas, such as：The requirement of the indexs such as sulphur, oxygen, nitrogen is extremely low, hence in so that most of product stills need import.
105624436 A of CN disclose one kind using chromium oxide as raw material, after with carbon, briquetting, using vacuum arc furnace ignition into
Row vacuum reduction, for the method due to using vacuum arc stove heat, control temperature fluctuation is big, causes product reaction incomplete, needs
Spray is carried out to product surface to sweep, remove the chromium trioxide on surface, product purity is only capable of reaching 99.5%, meanwhile, by equipment institute
Limit, can not large-scale production.
CN102965526 A disclose one kind using chromium oxide as raw material, after with carbon, briquetting, under elevated temperature in vacuo,
Reduction treatment, this method production cycle length, reduction are carried out to once sintered product using carbon monoxide, carbon dioxide and hydrogen
Property gas usage amount is big, and can not provide stable source of the gas, it is necessary to which secondary reduction, can not accomplish scale production.
1542148 A of CN 101660062 A and CN discloses one kind using chromium oxide as raw material, in elevated temperature in vacuo
Under, by secondary or once sintered production high-purity metal chromium, the method there are the problem of be that product consistency is low, and production capacity is small, no
It is adapted to industrialized production.
CN1102872C discloses a kind of method for removing nonmetallic inclusion, and this method is by raw material grind into powder, with height
Press mechanical pressing then passes to chromium powder briquet hydrogen, removes nonmetallic inclusion under the high temperature conditions, such as：C, O, S and N, the party
C, the O content of method are relatively low, but this method reaction time is grown, and hydrogen usage amount is big, and production cost is very high.
In conclusion the high-purity metal chromium produced using chromium oxide as raw material, due to the chemical property of raw material, with batch mixing and
Temperature controlled change, the segregation of usual carbon and oxygen element is very big, and product composition is uneven, and purity is low, can not be applied to high temperature
Alloy and target field.
The content of the invention
High temperature alloy is prepared the technical problem to be solved in the present invention is to provide a kind of compound degasser and target is special high-purity
The production method of crome metal, using compound degasser, preferably can remove the elemental gas in raw material, product impurity element pole
Low and uniform quality, can meet the requirement of high temperature alloy and high-end target.
The present invention technical solution be：
A kind of compound degasser prepares the production method of high temperature alloy and the special high-purity metal chromium of target, includes the following steps：
Step 1：By electrolysis produce crome metal piece crush after, through powder crushing process to granularity≤30 mesh powder, the metal
Fe ＜ 0.02% in chromium piece, Al ＜ 0.01%, Si ＜ 0.01%, oxygen ＜ 0.7%, sulphur ＜ 0.03%, then with compound degasser
Mixing, compound degasser are graphite-like reducing agent and the mixture of metal class desulfurization reducing agent, and incorporation time 4h~6h, is mixed
Material is closed, wherein, the weight ratio of the graphite-like reducing agent and the oxygen in crome metal piece is 0.75:1~0.9:1, metal class desulfurization
Reducing agent dosage is 3 times~5 times of raw material element sulphur quality；
Step 2：Above-mentioned mixture is pressed into Ф 30mm × (18 ± 2) mm billets, is then charged into square graphite material frame；
Step 3：Graphite material frame equipped with mixture billet is put into vacuum drying oven, is vacuumized, when vacuum in vacuum drying oven≤
Started to warm up during 5Mpa, temperature rises to 1400 DEG C~1600 DEG C, cools down after keeping the temperature 29h~35h, goes out when temperature is down to 170 DEG C
Stove, obtains the high-purity metal chromium product of chromium purity >=99.9%.
Graphite-like reducing agent described in step 1 is graphite powder, one kind in activated carbon, it is desirable to：Carbon content >=99.9%,
Granularity is -500 mesh, and the metal class desulfurization reducing agent in compound degasser selects one kind in Sn, Pb element, it is desirable to：Main grade
>=99.9%, the mesh of granularity -500.
The grinding particle size of the crome metal piece is 30 mesh, and require -200 mesh≤5%, with ensure mixing when material it is uniform
Property.
The pressure of the compacting billet of mixture can be effectively increased carbon dust and crome metal piece in 20MPa~25Mpa in step 2
Contact area, promote the reaction was complete.
Beneficial effects of the present invention：
(1), using the crome metal piece of electrolysis production as raw material, powder processed in the form of sheets and is beneficial to due to raw material, adds reactant
Contact area, the progress more conducively reacted, and by controlling suitable mixing time, uniform in quality.Before reaction, rationally control
Vacuum in vacuum drying oven processed, to reduce the oxygen content in material gap, improves product quality.The high-purity metal chromium of preparation need not
Double sintering, improves the purity of product and the utilization rate of recycling, and at present, which has accomplished scale production, and into
Work(is applied to high temperature alloy and target field.
(2) using the crome metal piece of electrolysis production as raw material, in the form of sheets, metals content impurity is low for appearance, gaseous impurity member
Element is concentrated mainly on surface, and wherein oxygen content is in 0.4%~0.7% (the mainly presence in the form of chromium hydroxide)；Sulfur content
Particle size range is easy to control in 0.01%~0.03%, its pulverizing process, improves the uniformity of batch mixing, meanwhile, in product
Elemental gas content be far below chromium oxide, by using the present invention compound degasser, can be preferably by the gas in raw material
Element of volume removes, and product impurity element is extremely low and uniform quality, and it is (mass percentage) to obtain product index：Cr >=99.9%,
Fe ＜ 0.02%, Al ＜ 0.01%, silicon ＜ 0.01%, C ＜ 0.012%, O ＜ 0.03%, can meet high temperature alloy and high-end
The requirement of target.
Embodiment
Embodiment 1
Step 1：30 mesh and the crome metal piece powder of -200 mesh≤5wt% are prepared through electrolysis production crome metal piece, weighs 2.5 tons
Crome metal piece powder, is 0.58wt% through analyzing its oxygen content, sulfur content calculates for 0.021wt% according to oxygen content, and addition is compound
Degasser 13.5kg, wherein：Graphite powder (carbon content >=99.9%, granularity are -500 mesh) 10.9kg, glass putty 2.6kg, Ran Houjin
Row mixing, incorporation time 4h, obtains mixture.
Step 2：Above-mentioned mixture is pressed into Ф 30mm × 16mm billets, suppresses the pressure of billet in 20MPa, then
Load in special graphite material frame；
Step 3：Above-mentioned material frame is put into vacuum drying oven, is started to warm up when vacuum reaches 4.2Pa in vacuum drying oven, temperature liter
To 1400 DEG C, start to cool down after keeping the temperature 29h, come out of the stove when temperature is down to 170 DEG C, obtain high-purity metal chromium product.
Products obtained therefrom is as follows through analyzing its each element component：
Embodiment 2
Step 1：50 mesh and the crome metal piece powder of -200 mesh≤5wt% are prepared through electrolysis production crome metal piece, weighs 2.5 tons
Crome metal piece powder, is 0.54% through analyzing its oxygen content, sulfur content calculates for 0.019% according to oxygen content, adds compound degassing
Agent 13.25kg, wherein：Graphite powder (carbon content >=99.9wt%, granularity are -500 mesh) 11.5kg, lead powder (main grade >=
99.9wt%, the mesh of granularity -500) 1.75kg, then mixed, incorporation time 5h, obtains mixture.
Step 2：Above-mentioned mixture is pressed into Ф 30*18mm billets, the pressure of billet is suppressed in 25Mpa, is then charged into
In special graphite material frame；
Step 3：Above-mentioned material frame is put into vacuum drying oven, is started to warm up when vacuum reaches 5.0Pa in vacuum drying oven, temperature liter
To 1450 DEG C, start to cool down after keeping the temperature 30h, come out of the stove when temperature is down to 170 DEG C, obtain high-purity metal chromium product.
Products obtained therefrom is as follows through analyzing its each element component：
Embodiment 3
Step 1：60 mesh and the crome metal piece powder of -200 mesh≤5wt% are prepared through electrolysis production crome metal piece, weighs 2.5 tons
Golden crome metal piece powder, is 0.54% through analyzing its oxygen content, and sulfur content 0.023%, calculates according to oxygen content, and addition is compound
Degasser 13.8kg, wherein：Active powdered carbon (carbon content >=99.9wt%, granularity are -500 mesh) 12kg, glass putty (main grade >=
99.9wt%, the mesh of granularity -500) 1.8kg, then mixed, incorporation time 4h, obtains mixture.
Step 2：Above-mentioned mixture is pressed into Ф 30*18 ± 2mm billets, suppresses the pressure of billet in 22Mpa, then
Load in special graphite material frame；
Step 3：Above-mentioned material frame is put into vacuum drying oven, is started to warm up when vacuum reaches 4.0Pa in vacuum drying oven, temperature liter
To 1600 DEG C, start to cool down after keeping the temperature 29h, come out of the stove when temperature is down to 170 DEG C, obtain high-purity metal chromium product.
Products obtained therefrom is as follows through analyzing its each element component：
It these are only the specific embodiment of the present invention, be not intended to limit the invention, for those skilled in the art
For member, the invention may be variously modified and varied.Any modification within the spirit and principles of the invention, being made,
Equivalent substitution, improvement etc., should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of compound degasser prepares the production method of high temperature alloy and the special high-purity metal chromium of target, it is characterized in that：
Include the following steps：
Step 1：By electrolysis produce crome metal piece crush after, through powder crushing process to granularity≤30 mesh powder, the metal
Fe ＜ 0.02% in chromium piece, Al ＜ 0.01%, Si ＜ 0.01%, oxygen ＜ 0.7%, sulphur ＜ 0.03%, then with compound degasser
Mixing, compound degasser are graphite-like reducing agent and the mixture of metal class desulfurization reducing agent, and incorporation time 4h~6h, is mixed
Material is closed, wherein, the weight ratio of the graphite-like reducing agent and the oxygen in crome metal piece is 0.75:1~0.9:1, metal class desulfurization
Reducing agent dosage is 3 times~5 times of raw material element sulphur quality；
Step 2：Above-mentioned mixture is pressed into Ф 30 × (18 ± 2) mm billets, is then charged into square graphite material frame；
Step 3：Graphite material frame equipped with mixture billet is put into vacuum drying oven, is vacuumized, when vacuum in vacuum drying oven≤
Started to warm up during 5Mpa, temperature rises to 1400 DEG C~1600 DEG C, cools down after keeping the temperature 29h~35h, goes out when temperature is down to 170 DEG C
Stove, obtains the high-purity metal chromium product of chromium purity >=99.9%.
2. compound degasser according to claim 1 prepares the producer of high temperature alloy and the special high-purity metal chromium of target
Method, it is characterized in that：Graphite-like reducing agent described in step 1 is graphite powder, one kind in activated carbon, it is desirable to：Carbon content >=
99.9%, granularity is -500 mesh, and the metal class desulfurization reducing agent in compound degasser is one kind in Sn, Pb element, it is desirable to：It is main
Grade >=99.9%, the mesh of granularity -500.
3. compound degasser according to claim 1 prepares the producer of high temperature alloy and the special high-purity metal chromium of target
Method, it is characterized in that：The grinding particle size of the crome metal piece is 30 mesh, and requires -200 mesh≤5%.
4. compound degasser according to claim 1 prepares the producer of high temperature alloy and the special high-purity metal chromium of target
Method, it is characterized in that：The pressure of the compacting billet of mixture is in 20MPa~25Mpa in step 2.
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| CN201711071630.8A CN107904410B (en) | 2017-11-03 | 2017-11-03 | A kind of compound degasser prepares the production method of high temperature alloy and the dedicated high-purity metal chromium of target |
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| CN201711071630.8A CN107904410B (en) | 2017-11-03 | 2017-11-03 | A kind of compound degasser prepares the production method of high temperature alloy and the dedicated high-purity metal chromium of target |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110453095A (en) * | 2019-09-17 | 2019-11-15 | 江苏隆达超合金航材有限公司 | The technique for removing impurity element in electrolytic metal chromium |
| CN116786810A (en) * | 2023-07-11 | 2023-09-22 | 涿州安泰六九新材料科技有限公司 | Chromium powder for sputtering target and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110453095A (en) * | 2019-09-17 | 2019-11-15 | 江苏隆达超合金航材有限公司 | The technique for removing impurity element in electrolytic metal chromium |
| CN116786810A (en) * | 2023-07-11 | 2023-09-22 | 涿州安泰六九新材料科技有限公司 | Chromium powder for sputtering target and preparation method thereof |
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| CN107904410B (en) | 2019-10-08 |
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Effective date of registration: 20221115 Address after: 121005 alloy No. 59, Taihe District, Liaoning, Jinzhou Patentee after: Jinzhou Vanadium Industry Co.,Ltd. Address before: 121005 alloy No. 59, Taihe District, Liaoning, Jinzhou Patentee before: CITIC JINZHOU METAL Co.,Ltd. |
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